CN109387551A - Manufacture method, ISE half-cell, sensor and the multi-parameter sensor of ISE half-cell - Google Patents
Manufacture method, ISE half-cell, sensor and the multi-parameter sensor of ISE half-cell Download PDFInfo
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- CN109387551A CN109387551A CN201810914486.8A CN201810914486A CN109387551A CN 109387551 A CN109387551 A CN 109387551A CN 201810914486 A CN201810914486 A CN 201810914486A CN 109387551 A CN109387551 A CN 109387551A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/31—Half-cells with permeable membranes, e.g. semi-porous or perm-selective membranes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/333—Ion-selective electrodes or membranes
- G01N27/3335—Ion-selective electrodes or membranes the membrane containing at least one organic component
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/301—Reference electrodes
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/302—Electrodes, e.g. test electrodes; Half-cells pH sensitive, e.g. quinhydron, antimony or hydrogen electrodes
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/403—Cells and electrode assemblies
- G01N27/413—Concentration cells using liquid electrolytes measuring currents or voltages in voltaic cells
Abstract
The present invention relates to method, ISE half-cell, sensor and the multi-parameter sensors of manufacture ISE half-cell.Disclose a kind of method for manufacturing ISE half-cell (1), the described method comprises the following steps: it includes in the coating solution (5) of at least one solvent and ion specific ion carrier that the first end of hollow body (3), which is immersed,；From the removal hollow body (3) in the coating solution (5)；The hollow body (3) is dried and evaporates the solvent from the coating solution (5), thus establishes ion-selective membrane (4) at the immersion end of the hollow body (3)；And the hollow body (3) is completed so that ISE half-cell (1) is made.The invention also discloses a kind of ISE half-cells (1) manufactured according to such method.The invention also discloses sensors (21) and multi-parameter sensor (25) including several such ISE half-cells (1).
Description
Technical field
The present invention relates to the method for manufacturing ISE half-cell, ISE half-cell, the sensors including such ISE half-cell
With the multi-parameter sensor including at least two ISE half-cells.
Background technique
The also referred to as ion-selective electrode of ion specificity electrode or ion-sensitive electrode (ISE) is served as specific molten
The concentration of the ion of solution or more specifically active sensor.In order to measure, by ion-selective electrode (the first half-cell) and
Second electrode (the second half-cell) i.e. reference electrode immerses in testing medium and measures the voltage between described two electrodes.Then
It can determine therefrom that sought concentration.Measured variable is the concentration dependent voltage to reference electrode.According to Nernst equation
Formula, the voltage depend on the activity of corresponding ion in logarithmic fashion.Most well-known ion-selective electrode be in response in proton (hydrogen from
Son or hydrogen ion) pH electrode.Ion-selective electrode uses in many fields, such as in the analysis including environmental analysis
Chemistry is used in biochemical and biophysics research and in the especially industrial process of process automation engineering.
The central module of ISE is ion-selective membrane, the ion-selective membrane will include electrode in electrode shell with to
Determining solution separates.The film has the ingredient changed dependent on ion to be determined.Most important film type is crystallization
Or vitreous solid, or the composite material with polymer.
The film is usually cast into flat film；Using polymer solution (such as with soft in the suitable solvent of such as THF
The PVC of agent and ionophore) it is used as cast-solution.After drying, fritter is cut or stamped out from basement membrane.These films are logical
It is often clamped or glued, they is installed (not bypass) in a fluid tight manner in the housing of ISE half-cell.
Lead to the pressurization of film as the non-clamping just cooperated, this may result in leakage in turn.When relatively short
In, due to settling, by the non-obvious loosening just cooperated of expection on mantle.In addition, the leaching of softening agent leads to the contraction of film.?
After longer standing time, the combination of the contraction of the sedimentation and film of film causes to bypass, this leads to the loss of measurement performance.In order to
The sedimentation and contraction of compensation film are necessary designing and manufacturing aspect clamping device at high cost.Clamping device includes can be with
Two film placement surfaces being displaced relative to each other.Described two film placement surfaces will must outwardly and inwardly seal tightly,
This makes it necessary to using different sealing elements.In addition, the contact pressure of two film placement surfaces must be with the consistency of film very
It matches well.Have to check for the impermeability of clamping device.
Adhesive may will affect the property of film, and cannot it is blood sure it be stable in the long term.It must be to viscous
Chalaza is pre-processed and checks whether it has impermeability.
Summary of the invention
It is as few as possible for using in the case where no additional method and step that the purpose of the present invention is to propose to a kind of
The manufacturing method of individual part manufacture ISE film.
The purpose is realized by method comprising the following steps: it includes at least one solvent that the first end of hollow body, which is immersed,
In the coating solution of ion specific ion carrier；Hollow body is removed from coating solution；Hollow body is dried and molten from film
Solvent is evaporated in liquid, thus establishes ion-selective membrane at the immersion end of hollow body；And hollow body (3) are completed so that ISE half is made
Battery (1).
Therefore, simple manufacturing method generates ISE half-cell on hollow body.Principle is based on molten via polymer is immersed
In liquid and dries and form film.The half-cell be characterized in that film with hollow body clearly and/or material connect, and do not have
Stress.
In order to influence the shape of film, exactly in order to which immersion is performed a plurality of times in one embodiment in the thickness for influencing film
With dry step.
In one embodiment, coating solution includes polymer solution.Coating solution therefore can also be by merging polymer
It establishes.In one embodiment, coating solution carries out special modification with the help of softening agent and solvent.
In one embodiment, it is modified that especially microcosmic surface is executed on hollow body, to improve adhesion strength.It is such to change
Property example be roughening, corona treatment, application tackifier, grinding, sandblasting, etching and/or coating.
In one embodiment, the hollow body with film is dipped into additional solution, it is especially antifouling to apply
The functional layer of layer or the layer for example by means of lotus-effect with low surface wettability ability.
In one embodiment, the method also includes the support construction for being especially metal is introduced on ion-selective membrane
Or it is introduced into the step in ion-selective membrane.Therefore the mechanical stability of film can be improved.Thus, for example being designed to grid
Support construction is located in film or on film.Support construction can also be designed by ceramics or plastics.Support construction can also be introduced into
Into functional layer.Support construction can also be introduced between film and functional layer, thus generate sandwich.
In one embodiment, the method also includes hollow body is being dipped into coating solution and is being moved from coating solution
Except after hollow body the step of the first end or second end of hollow body apply superpressure (overpressure).The superpressure is therefore
It can be positive pressure or negative pressure (" insufficient pressure (underpressure) ").
In one embodiment, it completes hollow body and includes at least following steps to manufacture ISE half-cell: by internal electrolyte
It is filled into hollow body, and reference electrode is introduced into the inside of hollow body.
In one embodiment, it completes hollow body and includes at least following steps so that ISE half-cell is made: hollow body is attached
The electrode axis of internal electrolyte can be extremely filled with.
In one embodiment, therefore replaceable housing is generated.
The purpose is also realized via according to the ion selection half-cell manufactured such as method presented above.
In one embodiment, hollow body includes at least one furrow (furrow), groove, indentation, rib, groove
(flute), recess, garland (undercut) etc., to increase adhesive surface or the positive cooperation (positive fit) of manufacture of film.
In one embodiment, on film, or in film, half-cell includes support construction, for example, by metal, plastics, can
Grid made of regrown material or ceramics.
In one embodiment, the internal diameter of hollow body is less than or equal to 10mm, is exactly less than 3mm.
In one embodiment, hollow body is fabricated by metal, glass, plastics or ceramics.
In one embodiment, the shape of film is designed to hemispherical or the shape as water droplet.Of course, it is also contemplated that its
Its film shape.
The purpose is also by including that just what a ion as described above selects the sensor of half-cell to realize.
In one embodiment, the outer diameter of sensor is less than or equal to 12mm.
In one embodiment, sensor also comprises reference half cell.
In one embodiment, sensor includes the plug for being connected to the especially induction type of transmitter.
The purpose is also by including that at least two ions as described above select the multi-parameter sensor of half-cell come real
It is existing.
In one embodiment, multi-parameter sensor also comprises reference half cell.
In one embodiment, multi-parameter sensor includes pH sensor, and multi-parameter sensor utilizes pH sensor
Reference half cell as its reference.
In one embodiment, multi-parameter sensor has the outer diameter less than or equal to 40mm.
Detailed description of the invention
This is explained in greater detail using the following drawings:
Fig. 1 a) to d) showing the claimed method for manufacturing film.
Fig. 2 a) and b) hollow body with garland or furrow is shown.
Fig. 3 a) to the embodiment for e) showing the ISE manufactured according to claimed method.
Fig. 4 shows one-parameter ISE.
Fig. 5 shows multi-parameter ISE.
Fig. 6 shows the multi-parameter ISE from Fig. 5, the upper part without shell.
Fig. 7 a) and b) hollow body before or after immersion is shown.
Fig. 8 shows the soaking hollow body being mounted in electrode axis.
Specific embodiment
In the accompanying drawings, identical feature is identified using identical reference symbol.
As it has been already mentioned, ISE half-cell 1 includes ion-selective membrane 4.For example, ISE half-cell 1 is to NH4 +、NO2 -、NO3 -、K+
Ion has selectivity.
Film 4 is formed via being dipped into hollow body 3 or immersing in the coating solution 5 with solvent；This aspect is referring to Fig. 1 a)
Or Fig. 1 b).Hollow body is made of glass, plastic tube, metal or ceramics.The internal diameter of hollow body 3 is approximately 1mm to 10mm, such as
For 3mm.Hollow body is approximately cylinder, or the polygonal profile with such as square profiles.
Coating solution 5 includes at least one solvent and an ion specific ion carrier.Polymer solution 5 especially includes example
Such as polymer solution and softening agent made of PVC (polyvinyl chloride).The solvent is, for example, THF (tetrahydrofuran).Polymer is molten
Liquid 5 is in room temperature, but impregnating can also be occurred with raised temperature or reduced temperature.Hollow body 3 is dipped into polymer
About 0.1s to 5s or longer time in solution 5.
(referring to Fig. 1 b) in next step), hollow body 3 is first drawn into polymer solution 5 (arrow b.in), and
Then extracted out (arrow b.out) from polymer solution 5.Fig. 1 b) in be symbolically illustrated in the appearance with polymer solution 5
Device.Film 4 forms and keeps this form by surface tension in extraction.
Film 4 is dried in next step；Referring to Fig. 1 c).Film 4 is for example being dried at room temperature；However, it is also possible to select higher
Or lower temperature.Solvent evaporates during drying process.
It can be impregnated by repetition with drying process in the case where changing and impregnating medium or soaking process and increase film thickness
Degree.
Therefore, if having used more solvents, viscosity can be changed by changing the ingredient of coating solution 5.Cause
This, can influence the shape and thickness that are formed by film 4.
The shape and thickness again may be by changing to the positive superpressure of application of hollow body 3 or negative superpressure.In a reality
It applies in example, the shape is in water droplet or hemispheric form.
Hollow body 3 can be via preceding --- being especially microcosmic ---, and surface is modified and is activated, on improving
The sticking property of the film 4 in face.It is thus regarded that surface is modified are as follows: roughening；Plasma treatment；Using tackifier, (such as surface is living
Property agent)；Grinding；Sandblasting；It etches (for example, by means of solvent, acid or caustic solution)；And/or coating.
Hollow body 3 can also include at least one furrow 10, groove, indentation, rib, groove, recess or garland 11 etc..Thus
Increase adhesive surface or generates additional positive cooperation.This aspect referring to fig. 2 a) or Fig. 2 b).
Via additional immersion or it can be immersed in additional solution 13 and apply additional functional layer 14.The layer 14 tool
There are anti-fouling effect or lotus-effect.This aspect is referring to Fig. 3.Therefore, Fig. 3 a)/Fig. 3 b)/Fig. 3 c) and in step and Fig. 1 a)/figure
1b)/Fig. 1 c) in those steps it is similar, i.e. the immersion, extraction and drying of polymer solution.It is empty in Fig. 3 d) in next step
Heart body 3 is dipped into additional solution 13 (arrow d.in), thus in extraction (arrow d.out) and drying (Fig. 3 e)) after,
Establish functional layer.
Especially metal, the grid of ceramics or plastics or the grid made of renewable raw material --- in general, branch
Support structure 12 --- it can be applied to film 4 or applied in film 4, to improve the mechanical stability of the film.In general, grid
Lattice are designed to support construction.Grid 12 can also be introduced between film 4 and functional layer 14, or only be introduced into functional layer 14
In.Grid 12 can also be specially introduced into functional layer 14.
By the suitable internal electrolyte of filling in inside 6 and with internal reference (for example, Ag/AgCl) and internal electrode
8 complete together to establish ISE half-cell 1；Referring to Fig. 1 d).ISE half-cell 1 is contacted via film 4 with medium 7 to be measured.
Ion-selective electrode is completed by connecting ISE half-cell 1 with reference half cell 2 via voltage measuring apparatus V.
Reference half cell includes external electrode 9, and the external electrode 9 is equally located in testing medium 7.
Method as described herein can be easily automated.
Fig. 8 shows Fig. 1 d) in for complete ISE half-cell embodiment alternative.Fig. 7 a) initially show it is hollow
Body 3.This is handled according to method as described above；Referring to Fig. 1 a), Fig. 1 b), Fig. 1 c), wherein generate come from Fig. 7 b) it is hollow
Body and film 4.Hollow body is attached to electrode axis 27.For example, this is carried out via the modes such as tightening, click, bond.
Therefore the replaceable housing for being used for electrode axis 27 is generated.
Fig. 4 shows one-parameter ISE sensor 21.Single parameter can be measured by means of sensor 21, the sensing
Device 21 is designed to one-parameter ISE.In this case, it is possible to parameter be NH4 +、NO3 -、NO2 -、K+、F-Or it is also possible to
Heavy metal ion.
Film 4 is visible in left end.Be arranged in 21 inside of sensor is ISE half-cell 1, has hollow body 3 and internal electricity
Pole 8.
Sensor 21 include correspond essentially to shown in reference electrode 9 (for example, Fig. 1 d)) reference electrode
24.It is the Ag/AgCl reference electrode contacted with internal electrolyte with reference to 24.Correspond to reference half cell 2 with reference to 24.Reference electrode
24 contact via diaphragm 24a with testing medium.For example, diaphragm 24a is PTFE diaphragm.
Sensor 21 has the outer diameter of 12mm.
Sensor 21 includes the plug 22 for example with induction type design.For this purpose, sensor 21 includes the corresponding ministry of electronics industry
Part, they relay the signal of ion-selective electrode 1 and reference electrode 24, and handle if necessary it.For this purpose, sensor
21 may include microcontroller.
Sensor 21 or its shell include the screw thread 23 for being mounted in frame, mounting bracket or flange.
Fig. 5 and Fig. 6 shows multi-parameter ISE sensor 25.Sensor 25 has shell, and the shell is with such as 40mm's
Diameter.Being located on the inside of it is at least two (for example, four) ions selection half-cell 1.These can be related to different ginsengs
Number, such as NH4 +、NO3 -、NO2 -、K+、F-Or there are also heavy metal ion.
Only the film 4 of electrode 1 is visible in Fig. 5.It is arranged in reference to 26 at the center of sensor 25.Certainly, different with reference to 26
It is fixed that central place is needed to arrange.In this example, with reference to being pH sensor.It preferably says, other than ion-selective electrode 1, passes
Sensor 25 further includes pH sensor.Other than pH non-sensitive part, pH sensor further includes reference electrode 26.For example, the reference
Electrode 26 is designed to the transfer of Ag/AgCl and internal electrolyte.The reference electrode 26 of pH sensor can be selected by ion
It is shared as reference electrode 9 to select electrode 1.
Sensor 25 or its shell include the screw thread 23 for being mounted in frame, mounting bracket or flange.
Sensor 25 includes the plug 22 for example with induction type design.For this purpose, sensor 25 includes the corresponding ministry of electronics industry
Part, they relay the signal of ion-selective electrode 1 and reference 26, and handle if necessary it.For this purpose, sensor 25 is also
It may include microcontroller.
List of numerals
1 ISE half-cell
2 reference half cells
3 hollow bodies
4 films
5 polymer solutions
61 inside
7 media
8 internal electrodes
9 external electrodes
10 furrows
11 garlands
12 grids
13 additional solution
14 functional layers
21 one-parameter ISE sensors
22 plugs
23 screw threads
24 references
24a diaphragm
25 multi-parameter ISE sensors
26 references
27 electrode axis
V voltage measurement
Claims (23)
1. method of the one kind for manufacturing ISE half-cell (1), the described method comprises the following steps:
The first end of hollow body (3) is immersed in the coating solution (5) including at least one solvent and ion specific ion carrier,
The hollow body (3) is removed from the coating solution (5) is middle,
The hollow body (3) is dried and evaporates the solvent from the coating solution (5), thus in the hollow body
(3) immersion end is established ion-selective membrane (4), and
The hollow body (3) is completed so that ISE half-cell (1) is made.
2. according to the method described in claim 1,
It is wherein performed a plurality of times and immerses step and drying steps.
3. method according to claim 1 or 2,
Wherein the coating solution (5) includes polymer solution.
4. according to claim 1 to method described at least one of 3,
The method also includes following steps:
It is modified that especially microcosmic surface is executed on the hollow body (3), to improve adhesion strength.
5. according to claim 1 to method described at least one of 4,
The method also includes following steps:
There to be the hollow body (3) of the film (4) to immerse in additional solution (13), it is special to apply functional layer (14)
It is not stain-proofing layer or the layer with low surface wettability ability.
6. according to the method described in claim 5,
The method also includes following steps:
The support construction (12) of especially metal is introduced on the ion-selective membrane (4) or is introduced into the ion-selective membrane
(4) in.
7. according to claim 1 to method described at least one of 6,
The method also includes following steps:
The hollow body (3) are being immersed in the coating solution (5) to and are being removed from the coating solution (5) hollow body
(3) apply superpressure after at the first end or second end of the hollow body (3).
8. according to claim 1 to method described at least one of 7,
Complete the hollow body (3) wherein ISE half-cell (1) is made and includes at least following steps:
Internal electrolyte is filled into the hollow body (3), and reference electrode (8) is introduced into the hollow body (3)
In internal (6).
9. according to claim 1 to method described at least one of 7,
Complete the hollow body (3) wherein ISE half-cell (1) is made and includes at least following steps:
The hollow body (3) is attached to the electrode axis (27) that can be filled with internal electrolyte.
10. a kind of as selecting half-cell (1) to the ion that method described at least one of 9 manufactures according to claim 1.
11. ion according to claim 10 selects half-cell (1),
Wherein the hollow body (3) includes at least one furrow (10), groove, indentation, rib, groove, recess, garland (11) etc.,
To increase the adhesive surface of the film.
12. the selection of ion described in 0 or 11 half-cell (1) according to claim 1,
Ion selection half-cell (1) includes the support construction (12) on the film (4) or in the film (4).
13. the selection of ion described at least one of 0 to 12 half-cell (1) according to claim 1,
Wherein the internal diameter of the hollow body (3) is less than or equal to 10mm, especially less than or equal to 3mm.
14. the selection of ion described at least one of 0 to 13 half-cell (1) according to claim 1,
Wherein the hollow body (3) is fabricated by glass, plastics or ceramics.
15. the selection of ion described at least one of 0 to 14 half-cell (1) according to claim 1,
Wherein the shape of the film (4) is hemispheric or in the form of water droplet.
16. a kind of including just what a selection of ion described at least one of 0 to 15 half-cell (1) according to claim 1
Sensor (21).
17. sensor (21) according to claim 16,
Wherein the outer diameter of the sensor (21) is less than or equal to 12mm.
18. sensor (21) described at least one of 6 or 17 according to claim 1,
Wherein the sensor (21) also comprises reference half cell (2,24).
19. sensor described at least one of 6 to 18 (21) according to claim 1,
Wherein the sensor (21) includes the plug (22) for being connected to the especially induction type of transmitter.
20. a kind of select half-cell (1) including ion described at least two according to claim 1 at least one of 0 to 15
Multi-parameter sensor (25).
21. multi-parameter sensor (25) according to claim 20,
The multi-parameter sensor (25) further includes reference half cell (2,26).
22. the multi-parameter sensor according to claim 20 or 21 (25),
Wherein the multi-parameter sensor (25) includes pH sensor, and the multi-parameter sensor (25) is passed using the pH
The reference half cell (2) of sensor refers to (26) as it.
23. the multi-parameter sensor according at least one of claim 20 to 22 (25),
Wherein the multi-parameter sensor (25) has the outer diameter less than or equal to 40mm.
Applications Claiming Priority (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102017118500 | 2017-08-14 | ||
| DE102017118500.3 | 2017-08-14 | ||
| DE102017128444 | 2017-11-30 | ||
| DE102017128444.3 | 2017-11-30 | ||
| DE102018102606 | 2018-02-06 | ||
| DE102018102606.4 | 2018-02-06 |
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| Publication Number | Publication Date |
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| CN109387551A true CN109387551A (en) | 2019-02-26 |
| CN109387551B CN109387551B (en) | 2021-12-07 |
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| Country | Link |
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| US (1) | US11460429B2 (en) |
| CN (1) | CN109387551B (en) |
| DE (1) | DE102018118792A1 (en) |
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| DE102018130183A1 (en) * | 2018-11-28 | 2020-05-28 | Endress+Hauser Conducta Gmbh+Co. Kg | Method of making an ISE half cell |
| DE102019114341A1 (en) * | 2019-05-28 | 2020-12-03 | Endress+Hauser Conducta Gmbh+Co. Kg | Method for checking the functionality of an ion-selective electrode assembly |
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- 2018-08-02 DE DE102018118792.0A patent/DE102018118792A1/en active Pending
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Also Published As
| Publication number | Publication date |
|---|---|
| US11460429B2 (en) | 2022-10-04 |
| US20190049402A1 (en) | 2019-02-14 |
| DE102018118792A1 (en) | 2019-02-14 |
| CN109387551B (en) | 2021-12-07 |
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